Effect of Calcination Temperature on the Structural and

Optical properties of ZnO Nanoparticles

Raminder Preet Pal Singh,1* I.S. Hudiara,2 Sudhakar Panday,3 Shashi Bhushan Rana4

1,3
Department of Electronics & Communication Engineering, Desh Bhagat University, Mandi Gobindgarh, India
2
Chitkara University (Punjab Campus), Chandigarh, India
4
Department of Electronics & Communication Engineering, GNDU Regional Campus, Gurdaspur, India
*
Corresponding author. Email: raminder_212003@rediffmail.com

Abstract

In the present study, ZnO nanoparticles were synthesized using a simple co-precipitation method with zinc acetate

and sodium hydroxide as precursor materials. The synthesized sample was calcined at 450 0C, 6000C and 7500C for

2h. The structural and optical properties of the ZnO samples were characterized by X-ray diffractometer (XRD),

Scanning electron microscope (SEM), energy dispersive spectroscopy (EDS) and UV-visible absorption

spectroscopy. The X-ray diffraction studies revealed that the as-synthesized ZnO nanoparticles have hexagonal

wurtzite structure. The average crystalline size was calculated using Debye-Scherrer’s formula. The particle size

was found to be in nano range and increases with increase in calcination temperature. SEM micro-image confirmed

the presence of spherical nanoparticles. EDS spectra shows highly pure ZnO nanostructures. UV-visible absorption

spectra shows slightly decrease in band gap with increasing calcination temperature.

Keywords: ZnO nanoparticles, Co-precipitation, X-ray diffractometer, Optical properties, UV-visible absorption

spectroscopy.

Introduction
ZnO is a group II-IV semiconductor and has become one of the most promising candidates for DMS materials. [5]

Moreover, ZnO have potential applications in optoelectronics due to its wide band-gap (3.3 eV) and high exciton

binding energy (60 meV) properties. Since zinc oxide shows different physical and chemical properties depending

upon the morphology of nanostructures, not only various synthesis methods but also the physical and chemical

properties of synthesized zinc oxide are to be investigated in terms of its morphology.

Most of the ZnO nanocrystals have been synthesized by traditional high temperature solid state reaction

method. However this method is time consuming and properties of the product can’t be controlled. ZnO
nanoparticles can be prepared on a large scale at low cost by simple solution based methods, such as chemical co-

precipitation, hydrothermal reaction, and sol-gel synthesis. In the present work, we have synthesized ZnO

nanoparticles using co-precipitation method. This is a simple and low cost method and gives good yield of the end

product and takes less time in preparing the nanoparticles. In this research work we have studied the effect of

calcination temperature on the structure and optical properties of ZnO nanoparticles.

Organization of this research paper is summarized as follows: Section 1, illustrate the experimental

procedure followed to synthesize the ZnO nanoparticles, followed by section 2, which describe the instrumentation

used to characterize the structural, morphological and optical properties of ZnO sample. In Section 3, various results

have been discussed in detail related to above said properties, while the Section 4 concludes the paper.

1. Experimental Procedure
All the materials used in this work were of analytical reagent grade and we have used them without any further

purification. In order to synthesize the pure ZnO nanoparticles, Zinc Acetate (Zn (CH 3COO) 2.2H2O), was dissolved

in distilled water and stirred for 1 hour. Aqueous solution of NaOH was added drop-wise to the solution to maintain

the pH ~10.The solution was then stirred at room temperature for 4 hours followed by aging for 24 hrs at the same

temperature. After aging, precipitate that formed was filtered and washed several times and was finally calcinated at

4500C, 6000C and 7500C for 2 hrs.

2. Characterization of pure and doped samples

X-ray diffraction patterns of all the powder samples were recorded by rotating angle X-ray diffractometer (Bruker

AXS D8 Advance, Germany) equipped with graphite monochromator, a mirror at a fixed incidence angle of 1-5°

and CuKα (Wavelength= 1.540 Aº, 40 KV, 100 mA) radiation source. The angular accuracy of the setup was 0.001º

and the angular resolution was about 0.01º. The samples were scanned in angular direction in the range from 20 to

90º (2θ) with step size of 0.01º. Surface morphology of undoped (pure) and doped synthesized samples was

ascertained by using scanning electron microscope Carl Zeiss Supras 55 which operates at a high accelerated voltage

of 15 kV. The UV absorption spectra of the samples were recorded on the Systronics-2205 double beam

spectrophotometer having bandwidth 1nm and wavelength ranges from 200-1100 nm. Elemental composition of

various sample were ascertained by using EDS spectroscopy at an acceleration voltage of 200 keV.
Results and discussions

XRD Analysis
Figure 1, shows X-ray diffraction patterns of the synthesized pure ZnO sample calcined at

different temperatures. Each XRD sample exhibit the hexagonal wurtzite phase without any

impurities and secondary phase formation. It is clearly from XRD pattern that all the

characteristic diffraction peaks can be indexed to the diffractions of (100), (002), (101), (102),

(110), (103), (200), (112) and (201) planes with a hexagonal wurtzite structure. These diffraction

peaks agree well within the values of the standard value of JCPDS no. 36-1451. XRD pattern

clearly shows that the intensity of peaks increases with increase in calcination temperature,

indicating increase in crystallinity at higher temperature.

Fig. 1. XRD patterns of ZnO calcined at different temperatures.

Table 1. Lattice & Optical Parameters of pure ZnO and Zn1−xCoxO (x = 0.01, 0.03 and 0.05) nanoparticles annealed at 600℃.
 Calcination Crystallite Size Absorption Band Gap
Temperature D (nm) Wavelength Energy
( OC ) (λ) (Eg)

450OC 31 nm Nm

600OC 33 nm Nm

750OC 42 nm nm

Scanning Electron Microscope (SEM) Analysis

Fig. 2. SEM image of

Table 2. EDAX data of Co-doped ZnO nanoparticle.

 Calcination Temperature
Zn % O%
( OC )

450OC 92.01 7.99

600OC 91.69 8.31

750OC 91.51 8.49

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